Hydrogenating unsaturated bodies.



C. ELLIS. HYDROGE NATING UNS ATUBATED BODIES. APPLICATION FILED MAR. 24,l9l6.

1 ,285,960. Patented Nov. 26, 1918.

' v In ven tor: m

CARLETON ELLIS, MONTCLAIR, NEW JERSEY.

HYDROGENATINGI. U'NSATURATED BODIES.

Specification of Letters Patent.

Continuation in part of application Serial No. 686,988, filed March 29,1912. This application filed March 24, 1916. Serial No. 86,522.

To all whom it may concern:

Be it known that I, CARLETON ELLIS, a citizen of the United States, anda resident of Montclair, in the county of Essex and State of New Jersey,have invented certain new and useful Improvements inthe Art ofHydrogenating Unsaturated Bodies, of which the following is aspecification.

The present invention relates to thehydrogenation of organic materialsby methods involvin the treatment thereof with hydrogen gas or gascontaining free hydrogen lybdenum,

in the presence of a hydrogen carrier comprising a colloidal non-noblemetal catalyst. This application contains matter disclosed in the fileof m former application Serial No. 656,100, filec October 23, 1911, nowLetters Patent No. 1,026,156, especially as-regards oil colloids orcolloidal catalyzers, as well as those catalyzers formed, for example,in situ by thermal decomposition, and is in part a continuation of mycopendin application 686,988, filed March 29, 1912 %now U. S. Patent No.1,217,118).

Among the various organic materials, in the treatment of which thepresent improvement is applicable, animal and vegetable'oils unsaturatedingredients, e. 9.,

containin cottonsee castor, linseed, Chinese wood, perilla, soy bean,peanut and fish oils; also crude or refined fatty acids, or other fattymixtures; a'lso wool grease, resins, especially ordinaryrosin,'naphthalene; tars and petroleum oils such as asphaltic oils andother as 'haltic bodies.

he object of the invention is to prevent deterioration of colloidalcatalysts of the nature of nickel especially (also applicable in thecase of cobalt, copper, iron and in some cases to chromium, manganese,titanium, vanadium) but generally to metals having atomic weightsbetween 48 and 63, which colloidal metals are extremely sensitive tovery small percentages .of oxygen. The invention is also applicable whenusing mothorium and zirconium in a state of extreme subdivision (e. g.colloidal metal) as the catalyst. I

- In view of the fact that small quantities, even minute traces ofoxygen are detrimental to the catalysts mentioned, I propose to avoidthe difficulty by avoiding the presence of oxygen in the system, andhence I employ, in the hydrogenation, hydrogen gas which is free fromoxygen.

perature, whereby catalytic The process may be carried out by contactlngthe organic material in' liquid state and the hydrogen in the presenceof the colloldal catalyst, at temperatures at which the catalyst 1seffective in producing a union of the hydrogen and unsaturatedcomponents of the organic material. This may be effected bycounter-current circulation, atomization, spraying or by bubbling thegas through the liquid, or in any other preferred manner.

As a specific example of my process, linseed oil, containing colloidalnicket catalyst to the extent of one per cent., while at a temperatureof between 150 and 200 (3., say 180 C., is treated in an apparatus suchas that shown in my Patent 1,138,201 (Figure 2) or that shown in myPatent 1,154,495 (Fig. 1, or Fig. 2) with hydrogen, in the entireabsence of free oxygen, and in the absence of materials having anypoisoning or other deleterious effect upon the catalyst. The operationmay be carried out under a pressure of, say, 10 to 25 1bs.-per squareinch, and under these conditions any nickel soap produced by the actionof the free fatty acid of the oil on the nickel catalyst, is quicklydecomposed.

The treatment is continued until the desired amount of hydrogen isadded, after which the catalyst is removed from the bulk of the oil forfurther use.

In order to produce the initial mixture of colloidal catalyst andorganic material, it is preferable to dissolve a readily reducible ordecomposable metallo-organic body in the organlc material in a liquidstate, and to decompose the same. As an example of this procedure, I maydissolve nickel oleate in an oil and then subject such mixture asflowing stream to the action of a counter current of hydrogen or watergas in the absence of free oxygen at an elevatadtemcolloidal nickel isproduced.

In many cases the presence of oxygen catalytic action usually exhibits astrong tendency to settle owing to some change in physlcal state.

It is preferable to remove dissolved oxygen fromthe oil beforehydrogenation, for

example by heating or by treating with hydrogen at an elevatedtemperature.

In the accompanying diagrammatic drawings, an illustrative form oftreating appabe packed with granular material of a nonmetallic nature,such for example, as granules of charcoal, or if desired, withnonmetallic material carrying or retaining a metallic oatalyzer, thenon-metallic material being active or inactive as the casemay be. Thetowers have bafiles in some cases and as shown at 3, the battles have alip which allows the gases to collect at the other side of the bafliesto form gas-pockets. 4 is the outlet for the gas discharging at 1, andthis gas may be carried back to the tower 2 and travel through thesystem in a cyclic path preferably after having been Washed. The ilenters at the inlet 5. 6 is a pressure gage. by steam coils throughwhich superheated steam may be passed. A pipe 7 leads from the lowerpart of the tower 1 to the upper part of the tower 2 and serves toconvey hydrogen gas from the latter to the former. An oil main runs fromthe top of the tank The tanks 1 and 2 are shown heated- 2 to the bottomof the tank 1. Hydrogen is generated in the electrolytic cell, 22 and isforcedby the pump 21 into the purifiers 19 and 17, inwhich it is freedfrom chlorin, then while substantially free from traces of oxygen gas,passes into the tower 2, moves upwardly therethrough and then is forcedinto the tower l where it travels upwardly in the same manner coming inintimatecontact with the oil which is flowing in. the opposite directionand being heated and if needful compressed to the point required for themost effective reaction. Finally any residual gases discharging at 4 maybe taken back to the pump 21 and used again inthe system in so far asthey may contain any useful hydrogen content.

The oil entering at 5 with or without a colloidal or finely dividedcatalyzer flows downwardly through the tower l and then is forced intothe tower 2 under a pressure sufficient to enable the oil to move freelyagamst the pressure of the hydrogen gas.

What I claim is chlorin.

. OARLETON ELLIS.

. v '55 In the process of hydrogenating organic

